215 resultados para ENERGY-ELECTRON DIFFRACTION


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CeF3 and CeF3:Tb3+ nanoparticles were prepared by reverse microemulsion with a functional monomer, methyl methacrylate (MMA), as the oil phase, and CeF3:Tb3+/poly (methyl methacrylate) (PMMA) nanocomposites were obtained via polymerization of the MMA monomer. The nanoparticles and nanocomposites have been well characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), low- and high-resolution transmission electron microscope (TEM), selected-area electron diffraction (SAED), thermogravimetric analysis (TGA), UV/vis transmission spectra, photoluminescence excitation, and emission spectra and luminescence decays. The well-crystallized CeF3 and CeF3:Tb3+ nanoparticles are spherical with a mean diameter of 15 nm. They show the characteristic emission of Ce3+ 5d-4f (313 nm, D-2-F-2(5/2); 323 nm, D-2-F-2(7/2)) and Tb3+ D-5(4)-F-7(J) (J = 6-3, with D-5(4)-F-7(5) green emission at 541 nm as the strongest one) transitions, respectively.

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Uniform lanthanide orthophosphate LnPO(4) (Ln = La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho) nanoparticles have been systematically synthesized via a facile, fast, efficient ultrasonic irradiation of inorganic salt aqueous solution under ambient conditions without any surfactant or template. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED), photoluminescence (PL) spectra as well as kinetic decays were employed to characterize the samples. The SEM and the TEM images show that the hexagonal structured lanthanide orthophosphate LnPO(4) (Ln = La, Ce, Pr, Nd. Sm, Eu, Gd) products have nanorod bundles morphology, while the tetragonal LnPO(4) (Ln = Tb, Dy, Ho) samples prepared under the same experimental conditions are composed of nanoparticles. HRTEM micrographs and SAED results prove that these nanostructures are polycrystalline in nature.

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Lutetium fluorides with different compositions, crystal phases, and morphologies, such as beta-NaLuF4 hexagonal microprisms, microdisks, mirotubes, alpha-NaLuF4 submicrospheres, LuF3 octahedra, and NH4Lu2F7 icosahedra, prolate ellipsoids and spherical particles have been successfully synthesized via a facile hydrothermal route. X-ray diffraction, scanning electron microscopy, transmission electron microscopy, high-resolution transmission electron microscopy, selected area electron diffraction, and photoluminescence spectra were used to characterize the samples. The intrinsic structural feature of lutetium fluorides, the solution pH values, F- sources, and organic additives (Cit(3-) and EDTA) account for the ultimate shape evolutions of the final products. The possible formation mechanisms for products with various architectures have been presented. Additionally, we investigated the upconversion luminescence properties of beta-NaLuF4: 20% Yb3+/2% Er3+ with different morphologies.

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Nearly monodisperse and well-defined one-dimensional (1D) Gd2O3:Eu3+ nanorods and microrods were successfully prepared through a large-scale and facile hydrothermal method followed by a subsequent heat treatment process, without using any catalyst or template. X-ray diffraction (XRD), thermogravimetric analysis and differential scanning calorimetry (TGA-DSC), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), selected area electron diffraction (SAED), photoluminescence (PL) and cathodoluminescence (CL) spectra as well as kinetic decays were used to characterize the samples. The size of the Gd2O3:Eu3+ rods could be modulated from micro- to nanoscale with the increase of pH value using ammonia solution. The as-formed product via the hydrothermal process, Gd(OH)(3):Eu3+, could transform to cubic Gd2O3:Eu3+ with the same morphology and a slight shrinking in size after a postannealing process.

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We report here a facile method to obtain folic acid (FA)-protected gold nanoparticles (Au NPs) by heating an aqueous solution of HAuCl4/FA in which FA acts as both the reducing and stabilizing agent. The successful formation of FA-protected Au NPs is demonstrated by UV/Vis spectroscopy, transmission electron microscopy (TEM), selected-area electron diffraction (SAED), X-ray photoelectron spectroscopy (XPS), and Fourier transform infrared spectroscopy (FTIR). ne intracellular uptake of these nanoparticles is facilitated by HeLa cells overexpressing the folate reporter, which itself is significantly inhibited by free FA in a competitive assay as quantified by inductively coupled plasma mass spectroscopy (ICP-MS). This simple one-step approach affords a new perspective for creating functional nanomaterials, and the resulting biocompatible, functional Au NPs may find some prospective applications in various biomedical fields.

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Stabilization effect on metastable phase II of isotactic polybutene-1 (iPB-1) by coated carbon has been investigated by transmission electron microscopy (TEM) and electron diffraction (ED) techniques. The results indicate that after evaporating carbon, the phase II-I crystal transformation time is greatly prolonged from 9 days for carbon-uncoated samples to 120 days for carbon-coated ones under atmospheric pressure, while under high pressure (50 bar), the phase transformation time increases from 5 min for the former to 20 min for the latter. The stabilization effect on metastable phase II of carbon coated iPB-1 is attributed to a surface fixing effect of the evaporated carbon.

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Syndiotactic polystyrene (sPS) nanorods of 200 and 80 nm diameters were prepared by infiltrating porous anodic alumina oxide templates with polymer melt, and the crystallinity and orientation of various forms of sPS crystals in the nanorods were studied by FTIR spectroscopy and electron diffraction. For sPS crystallized from amorphous state at lower temperatures, a-form crystals were found in the nanorods with random orientation and the same degree of crystallinity as that in the bulk. However, for sPS crystallized from molten state at 260 degrees C, while no preferred orientation was found for the chains in the melt, the beta-crystals formed in the nanorods oriented preferentially with the c-axis aligning perpendicular to the axial direction of the nanorod, and the degree of crystallinity was significantly lower than that in the bulk. The crystallinity decrease was more profound for nanorods of smaller diameter. These results were also supported by electron diffraction data and can be attributed to competition between nucleation and crystal growth in the nanotemplates.

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Morphology of synthetic imogolite nanotubes formed in droplet evaporation was investigated by transmission electron microscopy and electron diffraction. The nanotubes form a dense entangled network at higher concentrations, while at lower concentrations the nanotubes are liable to form oriented bundles. Under enthanol atmosphere, individual dispersion of nanotubes was observed for the first time, which reveals the length polydispersity of synthetic imogolite nanotubes.

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Single crystals of head-to-tail poly(3-hexylthiophene)s have been grown through the method of isothermal solution crystallization. Electron diffraction in combination with powder X-ray diffraction revealed the crystal structure, a = 1.52 nm, b = 3.36 nm, c = 1.56 nm and alpha = beta = gamma = 90 degrees.

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We developed an approach, i.e. solvent-assist crystallization (SAC), for growing high quality single crystals of head-to-tail regio-regular poly(3-butylthiophene) (P3BT). By means of atomic force microscopy, electron diffraction and X-ray diffraction, we found that P3BT macromolecules formed lamella single crystals through gradient crystallization, and in the single crystals, molecules packed normal to the lamella with extended-chain conformation with alkyl side chains in the growth front during crystallization.

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Nanowires of SiC were synthesized by carbothermally reducing PVP/TEOS composite fibres obtained by electrospinning. High-resolution transmission electron microscopy (HRTEM) and selected-area electron diffraction (SAED) indicated that the SiC nanowires are single crystalline in nature. Both Fourier-transformed infrared spectroscopy and HRTEM indicated that a thin layer of SiO2 was formed on the outer surface of the nanowire as a result of post-heat treatment for the removal of residual carbon. Such SiO2 layer protects the inner SiC fibre from further oxidation. The formation mechanism of single-crystalline SiC nanowires was proposed based on our understanding and characterizations. The growth of the nanowire is believed to be along the ( 111) of its cubic cell.

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BaF2 nanocrystals doped with 5.0 mol% Eu3+ has been successfully synthesized via a facile, quick and efficient ultrasonic solution route employing the reactions between Ba(NO3)(2), Eu(NO3)(3) and KBF4 under ambient conditions. The product was characterized via X-ray powder diffraction (XRD), scanning electron micrographs (SEM), transmission electron microscopy (TEM), high-resolution transmission electron micrographs (HRTEM), selected area electron diffraction (SAED) and photoluminescence (PL) spectra. The ultrasonic irradiation has a strong effect on the morphology of the BaF2:Eu3+ particles. The caddice-sphere-like particles with an average diameter of 250 nm could be obtained with ultrasonic irradiation, whereas only olive-like particles were produced without ultrasonic irradiation. The results of XRD indicate that the obtained BaF2:Eu3+ nanospheres crystallized well with a cubic structure. The PL spectrum shows that the BaF2:Eu3+ nanospheres has the characteristic emission of Eu3+ D-5(0)-F-7(J) (J = 1-4) transitions, with the magnetic dipole D-5(0)-F-7(1) allowed transition (590 nm) being the most prominent emission line.

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Polyethylene (PE) chains grafted onto the sidewalls of SWCNTs (SWCNT-g-PE) were successfully synthesized via ethylene copolymerization with functionalized single-walled carbon nanotubes (f-SWCNTs) catalyzed by rac-(en)(THInd)(2)ZrCl2/ MAO. Here f-SWCNTs, in which alpha-alkene groups were chemically linked on the sidewalls of SWCNTs, were synthesized by Prato reaction. The composition and microstructure of SWCNT-g-PE were characterized by means of H-1 NMR, Fourier transform infrared spectroscopy (FTIR), Raman spectroscopy, thermogravimetric analyses (TGA), field-emission scanning electron microscope (FESEM), and transmission electron microscope (TEM). Nanosized cable-like structure was formed in the SWCNT-g-PE, in which the PE formed a tubular shell and several SWCNTs bundles existed as core. The formation of the above morphology in the SWCNT-g-PE resulted from successfully grafting of PE chains onto the surface of SWCNTs via copolymerization. The grown PE chains grafted onto the sidewall of the f-SWCNTs promoted the exfoliation of the mass nanotubes. Comparing with pure PE, the physical mixture of PE/f-SWCNTs and in situ PE/SWCNTs mixture, thermal stability, and mechanical properties of SWCNT-g-PE were higher because of the chemical bonding between the f-SWCNTs and PE chains.

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The crystalline syndiotatic 1,2-polybutadiene was synthesized with a catalyst consisting of iron acetylacetonate (Fe(acac)(3))-triisobutylaluminum (Al(i-Bu)(3))-diethyl phosphite (DEP), and the effects of crystal growth conditions on morphology of thin films of the polymer were investigated by transmission electron microscopy (TEM) and electron diffraction (ED) techniques. The polymer with melting point 179 degreesC was found to have 89.3% 1,2-content and 86.5% syndiotacticity by C-13 NMR measurement. The results of electron microscopic studies indicate that the solution-cast thin films of the syndiotatic 1,2-polybutadiene consist of lath-like lamellae with the c-axis perpendicular to the film plane, while a- and b-axes are in the film plane. The morphology of isothermally crystallized thin films of the polymer is temperature dependent. At lower crystallization temperatures (130 degreesC), a spherulitic structure consisting of flat-on lamellae is formed. With an increase in the crystallization temperature (e.g., at 140 degreesC), the spherulites and single faceted crystals coexist. At higher crystallization temperatures (150 degreesC), single crystals with a hexagonal prismatic shape are produced.

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Micro-banded textures developed from thin films of a main-chain thermotropic liquid crystalline chloro-poly(aryl ether ketone) in the melt were investigated using transmission electron microscopy (TEM). selective area electron diffraction, and atomic force microscopy techniques. The micro-banded textures were formed in the copolymer thin films after annealing at temperatures between 320 and 330degreesC, where a highly ordered smectic crystalline phase is formed without mechanical shearing. The micro-banded textures displayed a sinusoidal-like periodicity with a spacing of 150 nm and an amplitude of 2 rim. The long axis of the banded texture was parallel to the b-axis of an orthorhombic unit cell. In the convex regions, the molecular chains exhibited a homeotropic alignment, i.e. the chain direction was parallel to the film normal. In the concave re-ions, the molecular chains possessed a tilted alignment. In addition to the effects of annealing temperatures and times, the thickness of the film played a vital role in the formation of the banded texture. A possible formation mechanism of this banded texture vas also suggested and discussed. It was suggested that the micro-bands were formed during cooling.